WO2018077781A1 - Procédé pour déterminer une propriété de perméation de faisceaux de membranes à fibres creuses - Google Patents
Procédé pour déterminer une propriété de perméation de faisceaux de membranes à fibres creuses Download PDFInfo
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- WO2018077781A1 WO2018077781A1 PCT/EP2017/076959 EP2017076959W WO2018077781A1 WO 2018077781 A1 WO2018077781 A1 WO 2018077781A1 EP 2017076959 W EP2017076959 W EP 2017076959W WO 2018077781 A1 WO2018077781 A1 WO 2018077781A1
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- WIPO (PCT)
- Prior art keywords
- hollow
- fiber membrane
- hollow fiber
- membrane bundle
- fiber membranes
- Prior art date
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- FDJOLVPMNUYSCM-WZHZPDAFSA-L cobalt(3+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(1r,2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2 Chemical compound [Co+3].N#[C-].N([C@@H]([C@]1(C)[N-]\C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C(\C)/C1=N/C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C\C1=N\C([C@H](C1(C)C)CCC(N)=O)=C/1C)[C@@H]2CC(N)=O)=C\1[C@]2(C)CCC(=O)NC[C@@H](C)OP([O-])(=O)O[C@H]1[C@@H](O)[C@@H](N2C3=CC(C)=C(C)C=C3N=C2)O[C@@H]1CO FDJOLVPMNUYSCM-WZHZPDAFSA-L 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
- B01D63/0233—Manufacturing thereof forming the bundle
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M1/00—Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
- A61M1/14—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis
- A61M1/16—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis with membranes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M1/00—Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
- A61M1/14—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis
- A61M1/16—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis with membranes
- A61M1/1621—Constructional aspects thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M2205/00—General characteristics of the apparatus
- A61M2205/33—Controlling, regulating or measuring
- A61M2205/3379—Masses, volumes, levels of fluids in reservoirs, flow rates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M2207/00—Methods of manufacture, assembly or production
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/04—Specific sealing means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/04—Specific sealing means
- B01D2313/041—Gaskets or O-rings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/42—Details of membrane preparation apparatus
Definitions
- the invention relates to a method for determining a permeation property of hollow fiber membranes in a hollow fiber membrane bundle.
- the invention relates to a method with which the ultrafiltration coefficient of hollow fiber membranes in a hollow fiber membrane bundle can be determined from a determined permeation property.
- the invention relates to an apparatus for carrying out a method for determining a Permeationseigenschaften, in particular the determination of the ultrafiltration rate, of hollow fiber membranes in a hollow fiber membrane bundle.
- the invention further relates to a process for producing hollow fiber membrane filter modules from hollow-fiber membranes having at least one predetermined permeation properties, in particular a predetermined ultrafiltration rate.
- Hollow fiber membranes are widely used in the purification of liquids.
- hollow fiber membranes are used in medical technology for water treatment and blood purification, especially in the dialysis of kidney patients.
- Corresponding hollow-fiber membranes are installed in hollow-fiber membrane bundles in filter modules. The production of such filter modules for blood purification is now carried out in mass production scale.
- the hollow fiber membranes used for the purification of blood are often composed of polysulfone (PSU) and polyvinylpyrrolidone (PVP) and are generally produced in a so-called "dry-wet" spinning process
- a spinning solution comprising the polymers PSU and PVP
- the spun filament is first passed vertically through an air space, the so-called precipitating gap, into which a coagulation medium is extruded into the lumen of the filament simultaneously with the extrusion of the filament, so that the extrusion of the filament
- the coagulation process leads to phase inversion, so that so-called sol and gel phases form within the spun yarn.
- the spun yarn, after passing through the precipitating gap is introduced into a precipitation bath in which the filament is completely precipitated and precipitated forming the solid hollow fiber membrane structure
- the resulting hollow fiber membrane passes through several rinsing baths and drying zones.
- PSU polymers containing sulfonic groups such as polyethersulfone and polyphenylsulfone and copolymers comprising these polymers.
- a multiplicity of hollow-fiber membranes are extruded simultaneously and in parallel in a production plant, so that the hollow-fiber membrane fibers obtained after passing through the production plant can be combined as a group of threads or fiber bundles and taken up by a reel.
- Corresponding methods are known in the prior art and described, for example, in DE 10 2006 057 101 A1.
- the manufacturing process of hollow fiber membranes is a continuous process that is operated in the production facilities in three-shift operation. It is therefore continually necessary to monitor the quality of the fibers produced in order to avoid larger production errors. Therefore, it is constantly checked whether the properties of the manufactured Hollow fiber membrane in the specified range and the production process according to the preset conditions expires.
- Hollow fiber membranes are characterized in particular by their permeation properties. On the basis of the permeation property of a hollow-fiber membrane, it has to be decided whether the hollow-fiber membrane is suitable for certain separation processes, e.g. in the dialysis of kidney patients, can be used. In order to determine a permeation property of hollow-fiber membranes, it has hitherto been necessary to construct filter modules from the hollow-fiber membrane bundles produced, on which it was then possible first to detect the separation properties of the membrane.
- the hollow fiber membrane bundles In filter construction, the hollow fiber membrane bundles must be formed in a filter housing and encapsulated end. The casting takes place with curable resin compositions, in particular with polyurethane. Potting itself and curing are time-consuming process steps, so it takes several hours to build the filter and the following analyzes on the filters in the production labs. During this time, the production of hollow fiber membranes continues. If in doubt, it may happen that the analysis results after a few hours show that the specifications of the manufactured hollow fiber membrane are no longer complied with, so that the production result of several hours must be discarded.
- the corresponding production result of hollow fiber membranes can be further processed into the corresponding filter modules.
- kidney filters are used for the blood purification of kidney patients.
- the blood purification of kidney patients is based on the principle of transmembrane mass transfer.
- blood is guided on the inside of the hollow-fiber membranes, while a corresponding dialysis fluid is guided on the outside of the hollow-fiber membranes.
- the flow direction of the liquids is opposite, so that a filtration using the countercurrent principle.
- unwanted metabolites such as urea, creatinine, phosphate and harmful plasma proteins are removed from the patient's blood by permeating them through the membrane wall and optionally being taken up by the dialysis fluid.
- dissolved constituents of the dialysis fluid can also permeate through the membrane wall to the blood side.
- the dialysis fluid is provided as an aqueous physiological solution containing eg electrolytes (eg Na + , K + , Mg 2+ , Ca 2+ , Cl " ), glucose and a buffer (eg NaHCO 3).
- electrolytes eg Na + , K + , Mg 2+ , Ca 2+ , Cl "
- glucose eg NaHCO 3
- a buffer eg NaHCO 3
- liquid and substances contained therein permeate through the membrane according to a transmembrane pressure gradient.
- the permeation of substances through the membrane occurs due to the molecular intrinsic motion of the solutes and a concentration gradient that exists across the membrane wall.
- the filtration process can be carried out according to one or the other type. If e.g.
- hollow-fiber membranes with large relatively large pores are used and / or high flow rates of the two liquid streams, blood and dialysate are preset, at least part of the filtration is convective.
- the ultrafiltration coefficient represents a further permeation property of hollow-fiber membranes.
- the ultrafiltration coefficient indicates, in a given filtration structure, the permeability of the hollow-fiber membrane to a liquid, generally water, per unit of time and pressure difference.
- Methods for determining the ultrafiltration coefficient of hollow fiber membranes are known in the art. In this regard, reference is made to the standard DIN / EN / ISO 8637: 2014. The standard describes the use of blood as a test fluid. However, as a modification of the standard, water or blood plasma is often used as the test fluid. In particular, water is widely available and measurement is greatly simplified. One therefore speaks of the "aqueous" ultrafiltration coefficient.
- Another object of the invention was to provide a device under the use of hollow fiber membrane bundles can be examined and the ultrafiltration rate of the hollow fiber membranes can be determined.
- a further object of the invention was also to provide a production process of hollow-fiber membranes which makes it possible to produce hollow-fiber membranes within a production process in such a way that the specifications of a permeation property of the hollow-fiber membranes, in particular the ultrafiltration rate, can be maintained.
- the invention relates to a method for producing hollow fiber membrane filter modules according to claim 21 using a method according to an embodiment 1 to 17.
- the above-mentioned object is achieved by a method for determining at least one permeation property, in particular the ultrafiltration rate, of hollow-fiber membranes.
- the method comprises the following steps: Providing a hollow fiber membrane bundle, comprising a plurality of hollow fiber membranes having a first end and a second end, wherein the lumens of the hollow fiber membranes at the first end of the hollow fiber membrane bundle open end, in particular liquid permeable and closed at the second end of the hollow fiber membrane bundle end, especially liquid-tight are,
- Determining a permeation property of the hollow fiber membranes It has been shown that it is possible with the aid of the specified method steps to determine permeation properties of hollow fiber membranes, without previously hollow-fiber membrane filter modules must be made from the hollow fiber membrane bundles. It thus eliminates the effort that has to be made available for the production of the test filter modules.
- the determination of the permeation property of the hollow fiber membrane is carried out without previously potting the hollow fiber membrane bundle.
- the method according to the invention comprises the following steps:
- a hollow fiber membrane bundle comprising a plurality of hollow fiber membranes having a first end and a second end, wherein the lumens of the hollow fiber membranes at the first end of the hollow fiber membrane bundle open end, in particular liquid permeable and on the second end of the hollow fiber membrane bundle closed at the end, in particular liquid-tight,
- At least one compression device for compressing the hollow fiber membrane bundle in at least one subregion (222, 322) of the hollow fiber membrane bundle, in particular of the subregion of the hollow fiber membrane bundle which adjoins the first end of the hollow fiber membrane bundle,
- the permeation property of the hollow fiber membranes can be determined without first having to prepare hollow fiber membrane filter modules from the hollow fiber membrane bundles. It thus eliminates the effort to be provided for the production of the test filter modules.
- hollow fiber membrane filter modules corresponding hollow fiber membrane bundles are formed in a housing of a filter module and encapsulated end with a casting resin in the housing.
- the space between the fibers is filled with the casting resin, so that no liquid at the end can penetrate the space between the fibers.
- the lumens of the hollow-fiber membranes are closed at the ends.
- the lumens of the hollow fiber membranes are exposed again by the end part of the grout is separated.
- the method according to the invention has the advantage that it is possible to dispense with the end-side encapsulation of the hollow-fiber membrane bundle.
- the hollow-fiber membranes only have to be closed at one end.
- an effect of the invention according to the first aspect is that the hollow-fiber membranes can be examined for their permeation property within a short time, ie within a few minutes after their production.
- Studies according to previous methods, which require the construction of complete test filter modules, take at least a period of 3 hours to complete. During this period, it may already come to a large waste production, which can be avoided with the inventive method.
- the method according to the invention thus has the advantage of providing results quickly and reliably for controlling the production of hollow-fiber membranes. As a result, larger production errors can be avoided
- the method consists of the following steps:
- a hollow-fiber membrane bundle comprising a multiplicity of hollow-fiber membranes having a first end and a second end, the lumens of the hollow-fiber membranes being open at the end, in particular liquid-permeable and end-capped at the second end of the hollow-fiber membrane bundle, in particular liquid-tight,
- At least one compression device for compressing the hollow fiber membrane bundle in at least one subregion (222, 322) of the hollow fiber membrane bundle, in particular the subregion of the hollow fiber membrane bundle which adjoins the first end of the hollow fiber membrane bundle .
- Determining the ultrafiltration rate and / or the ultrafiltration coefficient of the hollow-fiber membranes by taking at least one measured value, in particular by measuring the exiting amount of the at least one test liquid, on at least one liquid outlet.
- a hollow fiber membrane bundle comprising a plurality of hollow fiber membranes having a first end and a second end, wherein the openings of the lumens of the hollow fiber membranes at the first end of the hollow fiber membrane bundle open end, in particular liquid permeable, and at the second end of the hollow fiber membrane bundle closed at the end, in particular liquid-tight, are configured.
- the term "hollow-fiber membrane stabilizer” is understood to mean a bundle composed of a multiplicity of hollow-fiber membranes.
- the hollow fiber membrane is a membrane in the form of a hollow filament consisting of a porous material and having a substantially circular diameter
- the wall thicknesses of such hollow fiber membranes intended for dialysis can be, depending on the membrane material 10 to 100 ⁇ .
- Current lumen diameter of such hollow fiber membranes are between 150 ⁇ to 250 ⁇ , in particular between 180 ⁇ and 220 ⁇ , the fiber length is in the range of 150 ⁇ to 300 mm, in particular between 250mm and 300mm
- the cavity of hollow fiber membranes can be flushed through by liquids.
- hollow-fiber membranes to carry out substance separation, which takes place by utilizing a permeation of substances through a transmembrane mass transfer from the outside to the inner cavity, or from the inner cavity to the outside of the hollow-fiber membrane.
- Such hollow fiber membranes are typically used in therapeutic blood treatment.
- the material of the hollow-fiber membranes can be selected from polymers, preferably from polysulfone, polyethersulfone, polyvinylpyrollidone, polypropylene, polyacrylonitrile, polyamide, polyethylene ether, cellulose, cellulose regenerate, cellulose acetate or mixtures thereof.
- Particularly preferred are membranes comprising a hydrophobic polymer material, such as e.g. Polysulfone or polyethersulfone and a hydrophilic polymer material, such as e.g. Have polyvinylpyrrolidone, in particular consist thereof.
- the hollow-fiber membrane are configured in such a way that the membrane material has a plurality of pores which serve to facilitate a mass transfer between the interior of the hollow-fiber membrane and the environment surrounding the hollow-fiber membrane and, in particular, permits a selective mass transfer according to the size of the particles of the respective substances becomes.
- the hollow interior of the hollow fiber membrane is called "lumen".
- the term "lumen” is understood to mean a coherent cavity which extends in the interior of the hollow-fiber membrane lengthwise from the first end to the second end of the hollow-fiber membrane porous membrane wall so that liquids and / or gases passing through the interior of the lumen are in mass transfer contact with the membrane wall along the hollow fiber membrane and a transmembrane mass transfer can be observed. in particular to allow liquids and / or gases to flow into or out of the fiber interior.
- Hollow-fiber membrane bundles When joining a plurality of hollow fiber membranes to form a hollow fiber membrane bundles between the individual hollow fiber membranes between spaces through which also liquids and / or gases can be passed.
- One Hollow-fiber membrane bundles preferably have at least 50 to 20,000 hollow-fiber membranes. Typical diameters of hollow fiber membrane bundles are in the range of 15 mm to 50 mm.
- the hollow-fiber membrane bundle which is used in the method according to the invention is not cast, ie the ends of the hollow-fiber membrane bundle are not cast in a casting resin.
- the combination of a plurality of the hollow fiber membranes into a hollow fiber membrane bundle results in a packing of hollow fiber membranes in which the hollow fiber membranes abut one another in a density predetermined by the packing.
- Hollow fiber membrane bundles form a resistance in such a package. This means that a hollow fiber membrane bundle is compressible and builds up a restoring force when compressed. Compressed hollow fiber membrane bundles endeavor to return to a relaxed state. The restoring force is in particular also associated with a corrugation of the hollow-fiber membranes, which is used in the production of hollow-fiber membranes.
- Corresponding methods for producing hollow-fiber membranes and hollow-fiber membrane bundles are known from the prior art, for example from DE 100 07 327 A1.
- hollow-fiber membrane bundles as used in the method according to the invention, are characterized in that they have a first end and a second end, the first end being different from the second end.
- the hollow fiber membrane bundle has closed-end hollow fiber membranes at the second end.
- the openings of the lumens of the hollow-fiber membranes at the second end of the hollow-fiber membrane bundle are closed at the ends, in particular so closed, that no liquid and / or gas escape from the lumen into the environment at the end or enter the lumen from the environment.
- Methods for sealing the hollow fiber membranes at one end of the hollow fiber membrane bundle are known in the art.
- the hollow-fiber membranes can be closed by heat, for example by heat radiation or thermal contact, by resins, or by laser radiation. In the present case, a thermal contact method on an aluminum foil is preferred.
- a hollow fiber Membrane bundles are melted at the ends of the hollow fiber membranes on a hot plate at 250 ° C to 350 ° C on one side.
- an aluminum foil is positioned as a release film, which can be removed again after cooling from the end of the hollow fiber membrane bundle.
- the melting process on the heating plate fuses the openings of the lumens at the ends of the hollow-fiber membranes. This results in a liquid-tight closure at the first ends of the hollow fiber membranes.
- a housing for receiving the hollow-fiber membrane bundle having a first end and a second end, wherein the first end has at least one liquid inlet.
- housing is to be understood as meaning a hollow body which is intended to receive a large number of hollow-fiber membranes Housing, between the hollow-fiber membranes and between the inside of the housing and outside of the hollow-fiber membranes, which can be flowed through by liquids.
- Suitable housings can have an elongated extent, so that an extension axis of a housing is longer than a second and third extension axis and thus as the longitudinal axis of the housing According to the longitudinal extent of an intended housing, it can be used in preferred orientations, vertically and horizontally.
- a corresponding housing is cylindrical, for example designed as a sleeve.
- Corresponding sleeve-shaped housings may be open to at least one of the ends, so that a hollow-fiber membrane bundle can be introduced into the sleeve. Then the housing can be closed or combined with appropriate end caps or fittings.
- Corresponding sleeves which serve as casings for hollow-fiber membrane bundles, are known from the construction of dialyzers in the prior art.
- Corresponding housings are preferably made of a rigid plastic material, such as polycarbonate, polypropylene or Polyoxymethy- len or metals, such as stainless steel or aluminum.
- the housing has at least one first fluid inlet at one end of the housing.
- the liquid inlet is intended to allow liquid to flow into the interior of the housing and / or into the interior of the hollow-fiber membrane bundle or of the hollow-fiber membranes.
- the at least one liquid inlet may provide a cylindrical access to the housing at the one end of the housing.
- the fluid access can also represent an open end of a cylindrical housing.
- at least one liquid outlet is provided which is at a distance from the at least one liquid inlet. "Spaced" in the sense of the present application means that the liquid inlet and liquid outlet are so far apart that liquid flowing through the liquid inlet flows through a part of the housing and / or a part of the hollow fiber membrane bundle.
- At least one compression device is provided which is capable of compressing hollow-fiber membrane bundles in at least one partial region of the hollow-fiber membrane bundle.
- Hollow-fiber membrane bundles are characterized by being deformable and in particular compressible. During compression, the hollow fiber membranes in the hollow fiber membrane bundle are brought into a higher packing density.
- the packing density is to be understood as meaning the filling of hollow-fiber membranes in a hollow-fiber membrane bundle which has been introduced into a housing.
- the packing density of hollow fiber membranes is the sum of the cross-sectional areas of the individual hollow-fiber membranes divided by the total cross-sectional area which delimits all the hollow-fiber membrane cross-sectional areas in an array. As a rule, this is the housing cross-section.
- the packing density is calculated according to the following formula: d (fiber): is the mean outer diameter of the unloaded hollow fiber membrane d (Füter): is the inner diameter of the housing
- n is the number of hollow fiber membranes in the housing
- unloaded hollow fiber membrane means a single free hollow fiber membrane.
- the hollow fiber membranes can be deformed, i. Under load assume a deformed cross-section. In particular, this can result in packing densities of greater than 100%. For calculating the packing density, however, the diameter of the unloaded hollow-fiber membrane is always assumed.
- compression device an agent capable of increasing the packing density of the hollow fiber membranes in the hollow fiber membrane bundle is used.
- Compression devices with which hollow-fiber membrane bundles can be compacted are known in the prior art. These may be, for example, elastic rings which enclose a hollow fiber bundle at at least one point of the hollow fiber membrane bundle and compact the hollow fiber membrane bundle in accordance with an applied pretensioning of the elastic material of the rings. Furthermore, pressure cuffs or pressure pads can be placed around the hollow fiber membrane bundle or introduced into the hollow fiber membrane bundle, so that when the pressure cuff or the pressure pad is pressurized, the packing density of the hollow fiber membranes in the hollow fiber membrane bundle is increased.
- the hollow-fiber membrane bundles are pushed out of their position and brought into a compressed state by a special geometric configuration of the housing or parts of the housing, in particular by at least one liquid inlet or by at least one liquid outlet, thereby forming at least part of the hollow-fiber membrane bundle to compress.
- a special geometric configuration of the housing or parts of the housing in particular by at least one liquid inlet or by at least one liquid outlet, thereby forming at least part of the hollow-fiber membrane bundle to compress.
- This can be done for example by a mandrel and / or a sleeve, which is introduced into the center of the hollow fiber membrane bundle and parallel to the longitudinal axis of the housing.
- the at least one compression device is designed such that at least the portion of the hollow fiber membrane bundle, which adjoins the first open end, can be compressed.
- the hollow fiber membrane bundle is introduced into the housing by aligning the first end of the hollow fiber membrane bundle with the end open lumens of the hollow fiber membranes to the at least one first liquid inlet at the first end of the housing.
- the liquid inlet and the open ends of the lumens are disposed adjacent to the hollow fiber membranes, so that liquid communication between inflowing liquid and the open lumens of the hollow fiber membranes is present and the inflowing liquid penetrates into the inside of the hollow fiber membranes through the open lumens can.
- the introduction of the hollow fiber membrane bundle into the housing can take place with the aid of a low-friction intermediate film in which a hollow fiber membrane bundle to be examined is taken.
- the hollow-fiber membrane bundle hammered into the foil has a smaller diameter than the inner diameter of the housing so that the hammered-fiber bundle bundle can be inserted into the housing.
- the low-friction film which lies between the housing inner wall and the hollow-fiber membrane bundle can be pulled out, so that the hollow-fiber membrane bundle remains in the housing.
- An embodiment in which the hollow-fiber membrane bundle is partially compressed into the housing is preferred.
- the hollow-fiber membranes are largely space-filling according to the compression stress of the hollow-fiber membrane bundle and relax.
- the introduction of a hollow-fiber membrane bundle into a housing under compressive stress of the hollow-fiber membrane bundle, so that the hollow-fiber membranes largely fill the space of the housing is also referred to as a "shaping-in" of the hollow-fiber membrane bundle into the housing.
- test liquid is provided.
- 'Test liquid' means a liquid with which a membrane can be examined for a permeation property.
- test liquids may be, for example, aqueous solutions, pure water, blood plasma or blood.
- the test liquid is characterized in that it is membrane-permeable, or that at least part of the test liquid is membrane-permeable.
- the term "membrane-like" is to be understood as meaning that the test liquid or part of the test liquid can permeate from the lumen of the hollow-fiber membrane through the membrane wall into the outer environment of the hollow-fiber membrane
- any temperature can be selected in order to carry out the method according to the invention .
- temperatures of 10 ° C. to 90 ° C. are conceivable for carrying out the method, in particular temperatures of 20 ° C. to 40 ° C provided for the implementation of the method.
- At least one first test liquid is conducted through the at least one liquid inlet at the first end of the housing into the interior of the housing and / or the hollow-fiber membrane bundle and / or the hollow-fiber membranes.
- the intermediate space between the hollow-fiber membranes and the lumens of the hollow-fiber membranes are at least partially, preferably substantially completely, rinsed through.
- the hollow-fiber membrane bundle located in the housing is compressed in at least a partial region of the hollow-fiber membrane bundle by means of the at least one compression device.
- the partial region of the hollow-fiber membrane bundle is compressed, which adjoins the first end of the hollow-fiber membrane bundle.
- the compression causes an increase in the packing density of the hollow-fiber membranes in this partial area relative to the uncompressed partial area of the hollow-fiber membrane bundle.
- the compression thereby also causes a flow resistance in the space between the hollow fiber membranes. It is intended to adjust the compression so that a flow of liquid is largely prevented in the space between the hollow fiber membranes.
- the compressed portion of the hollow fiber membrane bundle in this case causes inflowing liquid at the first end of the housing penetrates into the interior of the housing in the open lumens of the hollow fiber membranes and the penetration of the liquid into the space between the hollow fiber membranes difficult, or is prevented.
- the compression must not be so strong that hollow-fiber membranes are damaged, in particular the liquid space in the lumens of the hollow-fiber membranes must not be impaired. However, a deformation of the hollow fiber membranes can be tolerated.
- the packing density is used for a given number and geometry of the hollow-fiber membranes. It has been found that a packing density of at least 80% in the compressed portion of the hollow fiber membrane bundle, at the input pressures of the test liquid provided for the method according to the invention, can effectively prevent the flow between the hollow fiber membranes. At packing densities of more than 150%, the hollow-fiber membranes, depending on the membrane material, are already in danger of being damaged.
- the packing densities in the compressed portion of the hollow fiber membrane bundle are in the range of greater than 80% to 150%, preferably 85% to 120%, more preferably 90% to 110%.
- the packing density in the uncompressed partial region of the hollow-fiber membrane bundle differs from the compressed partial region, since in this partial region a flow of liquid is required in the space between the hollow-fiber membranes.
- Packing densities in the non-compressed portion may range from greater than 20% to less than 70%. Above a packing density of 70%, the flow between the hollow-fiber membranes is already disadvantageously limited at a given necessary pressure of the incoming test liquid.
- the permeation property in particular the ultrafiltration rate and / or the ultrafiltration coefficient of the hollow-fiber membranes, is determined by measuring a measured value, in particular the amount of test liquid, at at least one liquid outlet, in particular per unit of time and based on the transmembrane pressure difference is obtained.
- Permeationseigenschafl of a membrane referred to in the context of the present application, the characteristic of a transmembrane mass transfer, the is associated with a permeation of a substance through a membrane wall.
- a permeation property of a membrane provides information about the pore structure of the membrane and is understood as a measure with which the membrane can be characterized in terms of its porous structure. Permeation observed through the transmembrane mass transfer is generally considered in relation to other quantities. In particular, for the purposes of the present invention, the term also means how much liquid can be separated by permeation across the membrane over a period of time. The amount of permeated liquid per unit time corresponds to the ultrafiltration rate.
- the ultrafiltration rate and the ultrafiltration coefficient are understood as a permeation property which describes a hollow-fiber membrane.
- the inventive method for the determination of the ultrafiltration rate in particular the ultrafiltration coefficient of the examined hollow fiber membranes can be used.
- the inflowing test liquid which hits the end of the hollow-fiber membrane bundle with the end-capped hollow-fiber membranes, to flow substantially only into the lumen of the hollow-fiber membranes and not into the space between the hollow-fiber membranes.
- the test liquid entered through the open ends of the hollow fiber membranes flows through the interior of the hollow fiber membranes. Because the ends of the hollow fiber membranes are closed at the second end of the hollow fiber membrane bundle, the test liquid in the non-compressed part of the hollow fiber membrane bundle permeates through the membrane wall as so-called ultrafiltrate into the space between the hollow fiber membranes.
- the space between the hollow fiber membranes is connected to the one further liquid outlet, so that the ultrafiltrate can be discharged from the housing.
- a permeation property of the hollow fiber membrane, in particular the ultrafiltration rate and / or the ultrafiltration coefficient by multiply or continuously measuring a measured value, in particular the amount of liquid which at least one liquid outlet during the inflow of the at least one Test liquid in the housing, accrued, added time-dependent, to obtain a time-dependent measured value course.
- the multiplicity of measured values recorded on a time-dependent basis, or the continuous course of measured values is suitable for compensating for measurement error fluctuations. If other process performance parameters are kept constant, e.g. Temperature or transmembrane pressure difference, so there is a linear correlation for the recording of the ultrafiltrate as a function of time. Accordingly, a linear regression line can be approximated to the course of the measured value and the ultrafiltration rate can be determined from the slope. Normalized to the preset constant transmembrane pressure difference, the ultrafiltration coefficient can be derived.
- the compressed part of the hollow fiber membrane bundle extends in the axial direction over a length of 10 mm to 150 mm measured from the first end of the hollow fiber membrane bundle.
- a length of 10 mm the compression of the hollow-fiber membrane bundle, depending on the packing density of the hollow-fiber membranes, does not provide a sufficient effect to suppress the flow of the test liquid in the space between the hollow-fiber membranes.
- the informative value of the measurement results as a quality feature for the construction of hemodialyzers is worsened, since the hollow-fiber membrane bundles in the production of dialysis filters themselves only have a length of approximately 250 mm to 300 mm.
- the at least one liquid outlet has a first and a second opening and the Flusstechniksauslass is attached to the housing so that a fluid connection between see the first opening in the non-compressed part of Hollow fiber membrane bundle lies and the second opening, which is located outside of the hollow fiber membrane bundle, is formed, wherein the liquid outlet extends in particular through the compressed portion of the hollow fiber membrane bundle.
- the at least one liquid outlet on the housing is constructed to penetrate the hollow fiber membrane bundle at the first end with the hollow fiber end-open membranes in axial alignment of the hollow fiber membranes, and compress the hollow fiber membrane bundle in that part of the hollow fiber membrane bundle.
- the liquid outlet takes the form of a sleeve.
- the liquid outlet serves as a compression device for the hollow fiber membrane bundle by displacing the hollow fiber membranes in the corresponding section of the hollow fiber membrane bundle, thus causing a higher packing density.
- the liquid outlet consequently establishes a fluid connection with the space between the hollow-fiber membranes in the non-compressed part of the hollow-fiber bundle, in order to discharge ultrafiltrate arising there.
- liquid outlet movably on the housing.
- the liquid outlet is moved in the axial direction to the longitudinal axis of the housing and pushed into a portion of the hollow fiber membrane bundle, so that the hollow fiber membranes are displaced from their position and the packing density is increased.
- the introduction of the liquid outlet into the hollow fiber membrane bundle can be carried out by means of an auxiliary means.
- the adjuvant may remain in the hollow fiber membrane bundle, or be removed after introduction of the liquid outlet According to this embodiment, it is provided to form the fluid nozzle in a mandrel-shaped manner or to form the fluid nozzle as a sleeve which is pushed into the hollow-fiber membrane bundle with the aid of a mandrel.
- a mandrel-shaped geometry causes the hollow-fiber membranes to be displaced without damage in order to increase the packing density in the compression region.
- it is provided to produce the compression of the hollow fiber membrane bundle by a combination of different compression devices. Accordingly, it can be provided the compression z.T. to produce by an inserted into the hollow fiber membrane bundle sleeve of Fiüsstechniksausiass and elastic rings or a pressure cuff.
- the packing density in the non-compressed part of the hollow fiber bundle is less than 70%.
- the terms “compressed” and “non-compressed” refer to portions of the hollow fiber membrane bundle which are at relatively different packing densities relative to each other. The terms are not necessarily to be understood as absolute terms. Accordingly, a portion of the hollow fiber bundle having a packing density of 60% can be understood to be uncompressed when a second portion of the hollow fiber membrane bundle has a packing density of 80%.
- At least one opening for venting is attached to the housing.
- a complete venting of the interior of the housing may be necessary.
- the housing may have the vent opening, for example as a perforated ring on the housing.
- the vent opening is arranged in the immediate vicinity of the end of the hollow-fiber membrane bundle, the hollow-fiber membranes of which are closed at the end. The vent can after the conditioning, ie after the housing has been vented, be closed again.
- At least one further opening in the housing opposite to the non-compressed section of the molded-in hollow fiber membrane bundle is provided, which lies in direct adjacency to the compressed section of the hollow fiber membrane bundle.
- At least one further liquid outlet is provided on the housing, opposite the compressed section of the molded-in hollow fiber membrane module, which lies in direct adjacency to the non-compressed section of the hollow fiber membrane bundle.
- the liquid outlet may be helpful in order to achieve complete flushing in the compressed section of the hollow-fiber membrane bundle during the conditioning process, ie during the flushing of the housing with test liquid before the start of measurement, even in the compressed part.
- a discharge of leakage fluid during the measurement is possible via this liquid outlet.
- leakage fluid designates test fluid which, despite the compression of the hollow-fiber membrane bundle, penetrates into the intermediate space between the hollow-fiber membranes.
- the further liquid outlet establishes a connection to the ambient pressure. Therefore, the pressure in the space between the hollow fiber membranes in the compressed portion of the hollow fiber membrane bundle drops to the level of the ambient pressure.
- the non-compressed portion is also related to the ambient pressure via at least one fluid outlet. Accordingly, any leakage liquid occurring in the space between the hollow fiber membranes in the compressed portion of the hollow fiber membrane bundle can not move beyond the further liquid outlet into the non-compressed portion of the hollow fiber membrane bundle because equalization of the pressure levels is achieved by the further liquid outlet.
- the compression of the hollow-fiber membrane bundle is effected in a partial region by at least two compression devices.
- one or more, in particular two compression devices can be mounted in the interior of the hollow-fiber membrane bundle.
- one or more compression devices, which at least partially surround the hollow-fiber membrane bundle, and one or more compression devices, which are located in the interior of the hollow-fiber membrane bundle can be provided.
- the compression by two compression devices has proven to be particularly advantageous in measurement methods on hollow fiber membranes with a large average pore size and high ultrafiltration coefficient.
- the occurrence of leakage fluid in the compressed partial region of the hollow-fiber membrane bundle can also occur, especially in the case of such hollow-fiber membranes, by ultrafiltration in the compressed partial region.
- a second compression device provides an improved barrier against the ingress of leakage fluid into the uncompressed portion of the hollow fiber membrane bundle.
- the at least one further liquid outlet is attached to the housing between the at least two compression devices.
- the pressure of the inflowing liquid is set to 50 mbar to 500 mbar, alternatively 100 to 300 mbar, alternatively 150 to 250 mbar. It has been shown that the ab described compression of the hollow fiber membrane bundle is sufficiently high to cause at the said pressures of the incoming test liquid sufficient blocking effect of the flow in the space between the hollow fiber membranes.
- the pressures can thus be selected sufficiently high to produce a sufficiently high transmembrane pressure gradient for the determination of the ultrafiltration rate.
- the ultrafiltration rate can then be determined from the amount or the volume of ultrafiltrate which is obtained per unit time at the liquid outlet.
- the volume of ultrafiltrate can be determined volumetrically or gravimetrically based on the density of the test liquid by conventional methods.
- the ultrafiltration rate values determined by standardized methods e.g. DIN / EN / ISO 8637: 2014, deviate.
- the measured values obtained can be corrected by means of previously determined calibration values or by means of a calibration function.
- the invention relates to an apparatus for carrying out a method according to one of the embodiments according to the first aspect of the invention.
- the device is a measuring device with which a permeation property, in particular the ultrafiltration rate and / or the ultrafiltration coefficient of hollow-fiber membranes, on a hollow-fiber membrane bundle can be determined.
- the device comprises:
- a housing having a first end and a second end for receiving a hollow fiber membrane bundle, the first end of the housing having at least one liquid inlet,
- At least one connecting device for feeding the at least one test liquid from the at least one reservoir into the interior of the housing and / or the hollow-fiber membrane bundle, and / or the hollow-fiber membranes.
- At least one compression device for compressing at least a portion of the hollow fiber membrane bundle
- • means for time-dependent measurement of a permeation property, in particular the ultrafiltration rate and / or the ultrafiltration coefficient at at least one liquid outlet.
- the device according to the invention has the advantage that hollow-fiber membrane bundles can be examined with regard to their permeation property, in particular with regard to the ultrafiltration rate and / or the ultrafiltration coefficient, without the hollow-fiber membrane modules having to be cast into test filter modules and having to be installed as filter modules.
- hollow-fiber membrane bundles within a few minutes with respect to one of their Permeation property, in particular with regard to the ultrafiltration rate and the ultrafiltration coefficient.
- the device is therefore particularly suitable for monitoring the product specifications of the hollow fiber membranes produced in terms of one of the predetermined permeability properties in the continuous production of hollow-fiber membranes.
- the device furthermore has means for determining the pressure at at least one liquid inlet.
- Corresponding means are known in the art and may e.g. represent a pressure sensor.
- the pressure sensor By means of the pressure sensor, the inlet pressure of the incoming test liquid can be determined at the at least one liquid inlet.
- a pump which conveys the test liquid to the at least one liquid inlet, a predetermined pressure of the inflowing test liquid can be adjusted.
- a further means for determining the pressure in particular a pressure sensor, may be provided on the at least one further liquid outlet in order to determine the exact transmembrane pressure difference.
- the pressure at a liquid outlet corresponds to the ambient pressure, so that the recorded pressure value at the at least one liquid inlet is sufficient for determining the transmembrane pressure difference.
- the determination of the transmembrane pressure difference is necessary for the determination of the ultrafiltration coefficient from the measured ultrafiltration rate.
- the housing in an end-side part which is provided for receiving the portion of the hollow fiber membrane bundle with the end-closed hollow fiber membranes, at least one gas outlet.
- the gas outlet can serve as a vent opening through which the air separated during the measuring process can be diverted.
- the housing has at least one opening as a gas inlet in a section which is provided for receiving an uncompressed part of the hollow-fiber membrane bundle.
- the gas inlet may serve to introduce air into the interior of the housing if necessary. With the aid of the introduced air, an air flow can be formed in the housing in order to discharge accumulating permeate, in particular ultrafiltrate, in the intermediate space between the hollow-fiber membranes to the liquid outlet. The more accurate the measurement, the better the water flows on the respective membrane sides can be separated. Consequently, it is important that as much of the ultrafiltrate as possible is directed inward toward the central fluid outlet.
- the invention in a third aspect relates to the use of a device according to the invention according to the second aspect of the invention for applying a method according to the invention according to the first aspect of the invention.
- the invention relates to the production of hollow fiber membrane filter modules, wherein the inventive method according to an embodiment of the first aspect of the invention is used to produce hollow fiber membrane having a predetermined permeation property.
- the production process of hollow fiber membrane filter modules according to the invention comprises the following steps:
- step (b) selecting one or more manufacturing parameters to produce hollow fiber membranes having the at least one permeation property, or the plurality of permeation properties, with the range of values specified in step (a),
- step (c) preparing hollow fiber membranes by a spinning process according to one or more manufacturing parameters selected in step (b),
- step (f) using the hollow fiber membrane bundles for the construction of filter modules, if it is determined that the one or more permeation properties are in the range of values defined in step (a).
- a permeation property, in particular the ultrafiltration rate and / or the ultrafiltration coefficient of the hollow fiber membranes produced can be determined in a short time, the production process of hollow fiber membrane filter modules can be controlled in a timely manner. In particular, it can be checked whether the hollow fiber membranes produced correspond to the specified product specification, so that the hollow fiber membranes can be released for the construction of hollow fiber membrane filter modules.
- the production parameters can subsequently be adapted so that the hollow fiber membranes obtained correspond again to the product specifications.
- the thus regulated manufacturing process then goes back through the intended steps (a) to (f), in which it can be decided for the produced hollow fiber membranes to use these for the construction of the hollow fiber membrane filter modules.
- the preparation process of the invention is particularly suitable for the production of hollow fiber membrane filter modules, which are produced on the basis of the membrane materials polysulfone (PSU) and polyvinylpyrrolidone.
- the spinning solution used to make such hollow fiber membranes contains polysulfone (PSU) and polyvinylpyrrolidone (PVP) dissolved in a polar aprotic solvent.
- Suitable solvents are, for example, N-methyl-pyrrolidone, dimethyl sulfoxide or di-methyl-acetamide. It has been found that in the case of mixtures of polysulfone / polyvinylpyrrolidone spinning solutions it is particularly difficult to precisely adjust the permeation properties, in particular the ultrafiltration rate and / or the ultrafiltration coefficient, of hollow-fiber membranes, since these react very sensitively to fluctuations in the production parameters.
- the present inventive production process has proven to be particularly advantageous for the production of PSU / PVP hollow-fiber membranes, since it offers the possibility to detect deviations caused by the change in the production parameters in the shortest possible time and to adapt the production process accordingly.
- FIG. 1 is a schematic representation of a device according to the invention for determining the ultrafiltration rate and / or the ultrafiltration coefficient of hollow-fiber membranes of a hollow-fiber membrane bundle.
- the measuring device (100) has a measuring chamber (101), a water bath (102) in which distilled water tempered to 37 ° C. is presented as test liquid, a pump (103) with which the water is conveyed into the measuring chamber (101), a flow meter (104), and a pressure sensor (105).
- the pump is controlled so that the water flowing into the device (100) has a constant inlet pressure of 200 mbar.
- the amount of water supplied is always determined with a flow meter (104).
- FIG. 2 is a more detailed schematic representation of the measuring device (200) according to the invention with the following designations:
- a hollow fiber membrane bundle is formed in the housing sleeve (202) of the measuring chamber.
- the housing consists in this embodiment of a sleeve (202), which is followed by a receiving part (203), and a sleeve-shaped liquid outlet (204) into which a mandrel (205) is inserted.
- the receiving part (203) has a liquid inlet (212).
- the housing sleeve (202) is inserted at one end in the receiving part (203) and is sealed with 2 O-rings (206).
- the housing is provided with 3 pegs.
- the pimples form gas outlet (207), gas inlet (208) and the further liquid outlet (209) to remove leakage water.
- the test liquid used is water.
- a displaceable mandrel (205) with the sleeve enclosing the mandrel is designed as a liquid outlet (204) which extends into the fiber bundle (220).
- the mandrel (205) can be removed again.
- the sleeve-shaped liquid outlet (204) remains in the hollow-fiber membrane bundle (220).
- the hollow-fiber membrane bundle has a non-compressed section (221) in the upper region, in which no mandrel (203) and / or liquid outlet (204) is located, and a compressed section (222) in the lower region.
- FIG. 3 is a further schematic representation of a measuring device (300) according to the invention, which is essentially identical to the measuring chamber of FIG. 2.
- the following terms apply: • housing (301)
- Fig. 3 shows an embodiment with a liquid outlet (340), which is located in the hollow fiber membrane bundle.
- a first end (341) of the liquid outlet is in the portion of the hollow fiber membrane bundle which is not compressed (321).
- the second end (341) of the liquid outlet is external to the measuring device (300) so that fluid communication is established with the space between the hollow fiber membranes in the uncompressed portion (321) of the hollow fiber membrane bundle (320) and the outside of the measuring device (300).
- the leaking water from the lower perforated ring (309) of the sleeve is fed back into the water basin.
- the auxiliary air can be supplied by means of a sleeve at the gas inlet (308).
- the gas outlet (307) can be opened or closed as desired.
- FIG. 4 shows a schematic representation of a further embodiment of the device according to the invention, with an alternative compression devices with the flow of educallkeit in the space between the hollow fiber membranes can be prevented.
- the following designations apply to FIG. 4: Housing (401)
- Fig. 4 shows two hollow fiber membranes (420, 421) which are schematically for a plurality of hollow fiber membranes of a hollow fiber membrane bundle and which are liquid-tightly closed at one end (422). 4 further shows a first compression device 450 and a second compression device 451 enclosing the hollow fiber membrane. Furthermore, a third compression device (460) is mounted within the hollow fiber membrane bundle symbolized by the hollow fiber membranes (420, 421). A fourth compression device (461) is also located within the hollow fiber membrane bundle. In one embodiment, it may be provided that one or more compression devices (450, 451) are mounted enclosing the hollow-fiber membrane bundle.
- the undulating pattern of the hollow fiber membranes (420, 421) schematically represents the compression of the hollow fiber membrane bundle caused by the compression devices (450, 451, 460, 461).
- the first and third compression devices (450, 460) as well as the second and fourth compression devices (451, 461) are mounted substantially at the same height on the hollow fiber membrane bundle, that is, face each other.
- the four arranged compression devices divide the hollow fiber membrane bundle into three areas (A, B, C).
- the region C is in communication with the liquid inlet (412).
- the region A communicates with a liquid outlet (440).
- the pressure in region C prevails in the lumen of the hollow-fiber membranes Liquid is higher than in the space between the hollow fiber membranes in the area A, takes place an ultrafiltration of test liquid through the membrane wall from the lumen side of the hollow fiber membranes into the gap of the hollow fiber membranes in the area C.
- the compression device (451) and / or (461) By compressing the hollow-fiber membrane bundle by means of the compression device (451) and / or (461), a flow of incoming test liquid in the intermediate space between the hollow-fiber membranes from region C into region B is largely prevented.
- the accuracy of the measurement requires that the leakage fluid be removed.
- area B is separated from area A by another compression device and area B communicates with another liquid outlet (409).
- another liquid outlet (409) about the other liquid outlet (409), a pressure in the space between the hollow fiber membranes, which corresponds to the ambient pressure.
- the water bath (102) is filled up with distilled water and heated to 37 ° C.
- the fiber bundle to be examined is melted with the aid of an aluminum foil on a hotplate at about 300 ° C. on one side.
- the thus treated hollow fiber membrane bundle (220, 320) is molded into the housing sleeve (201, 301).
- the housing sleeve (201, 301) is now introduced into the receiving part (202, 303).
- the mandrel (205) is pressed together with the sleeve enclosing the mandrel (204, 340) until it stops in the fiber bundle (220, 320). Subsequently, the mandrel (205) is pulled out and the sleeve (340) remains in the bundle.
- An air sleeve is attached to the perforated ring of the gas inlet (208, 308) and fed to a small air flow.
- the perforated ring of the gas outlet (207,307) is closed.
- the pump is switched on. After conditioning, i. After a pumping process of 5 or 10 minutes, depending on the type of membrane, the ultrafiltrate is collected in a container and weighed at defined measuring times. The ultrafiltration coefficient can be calculated with the aid of the measured transmembrane pressure.
- the ultrafiltration rate is measured directly on the hollow-fiber membrane bundle to be examined (220, 320), without the hollow-fiber membrane bundle having to be cast and installed in a filter module for this purpose.
- a very strong flow resistance is created in the space between the hollow fiber membranes.
- a flow in the region of this flow resistance which corresponds to the compressed part of the hollow-fiber membrane bundle in the housing (222, 322), largely prevented.
- the generated flow resistance thus provides the same effect as an otherwise conventional encapsulation, by liquid flow between the hollow fiber membranes is prevented, the end open hollow fiber membranes remain accessible but inflowing liquid, and so liquid can enter the lumens of the hollow fiber membrane bundle.
- the hollow-fiber membrane bundle (221, 321) formed in the housing of the measuring device (100, 200, 300) is flushed through with test liquid for the measurement procedure.
- the test liquid is flowed through the liquid inlet (212, 312) into the measuring device (100, 200, 300), in particular into the receiving part of the housing (203, 303) and the inlet pressure is set to 200 mbar.
- the inlet pressure can be adjusted by means of pressure gauge (105) and pump (103).
- the inlet pressure adjusts in the receiving part and on the lumen side of the hollow-fiber membranes over the entire length of the hollow-fiber membrane.
- the test liquid can pass only through the transmembrane transition into the space between the hollow fiber membranes in the portion of the uncompressed part (321) of the hollow fiber membrane bundle. In this transition, a pressure gradient forms, so that in the space between the hollow fiber membranes in the non-compressed part (321), a water pressure prevails, which corresponds to the ambient pressure.
- the water produced by ultrafiltration in the space between the hollow-fiber membranes flows out through the (340) liquid outlet.
- the transmembrane pressure gradient causes ultrafiltration.
- the water present by ultrafiltration in the interstices between the hollow fiber membranes is directed to the central liquid outlet (304). This is done by the gas inlet (308), through which an air flow is introduced into the housing.
- the hole circle for the auxiliary air is attached to the housing sleeve (302) in such a way that the water droplets that can form in the hollow fiber membrane bundle (220, 320) are guided from outside to inside to the first end (341) of the fluid outlet (340) and discharged become.
- a section of the molded hollow fiber membrane bundle is deformed so strongly by means of the mandrel (205) and the sleeve-shaped liquid outlet (204, 340) that a maximum flow resistance is obtained between the hollow-fiber membranes without hollow-fiber membranes to damage. Due to the displacement of the hollow-fiber membranes, the packing density in the compressed section of the hollow-fiber membrane in the present application example increases from about 60% to about 95%.
Abstract
L'invention concerne un procédé pour déterminer une propriété de perméation de membranes à fibres creuses, la propriété de perméation de la membrane à fibres creuses étant déterminée sur un faisceau de membranes à fibres creuses qui est introduit dans une enveloppe, ledit faisceau de membranes à fibres creuses comprenant, à une première extrémité, des membranes à fibres creuses ouvertes du côté de l'extrémité et, à une seconde extrémité, des membranes à fibres creuses fermées du côté de l'extrémité. Sous l'effet de la compression radiale du faisceau, les espaces entre les fibres au niveau des extrémités ouvertes du faisceau sont fermés sans qu'il soit nécessaire de sceller le faisceau. L'invention concerne en particulier un procédé pour déterminer le taux d'ultrafiltration et/ou le coefficient d'ultrafiltration de membranes à fibres creuses.
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2019521642A JP7232179B2 (ja) | 2016-10-24 | 2017-10-23 | 中空糸膜束の透過特性を決定する方法 |
EP17787409.6A EP3528932B1 (fr) | 2016-10-24 | 2017-10-23 | Procédé et système pour déterminer une propriété de perméation de faisceaux de membranes à fibres creuses |
CN201780066024.9A CN109890485B (zh) | 2016-10-24 | 2017-10-23 | 用于确定中空纤维膜束的渗透性能的方法 |
US16/343,415 US11052350B2 (en) | 2016-10-24 | 2017-10-23 | Method for determining a permeation property of hollow fibre membrane bundles |
US17/358,025 US11541355B2 (en) | 2016-10-24 | 2021-06-25 | Method for determining a permeation property of hollow fibre membrane bundles |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE102016012722.8A DE102016012722A1 (de) | 2016-10-24 | 2016-10-24 | Verfahren zur Bestimmung einer Permeationseigenschaft von Hohlfasermembranen |
DE102016012722.8 | 2016-10-24 |
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US16/343,415 A-371-Of-International US11052350B2 (en) | 2016-10-24 | 2017-10-23 | Method for determining a permeation property of hollow fibre membrane bundles |
US17/358,025 Continuation US11541355B2 (en) | 2016-10-24 | 2021-06-25 | Method for determining a permeation property of hollow fibre membrane bundles |
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WO2018077781A1 true WO2018077781A1 (fr) | 2018-05-03 |
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PCT/EP2017/076959 WO2018077781A1 (fr) | 2016-10-24 | 2017-10-23 | Procédé pour déterminer une propriété de perméation de faisceaux de membranes à fibres creuses |
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US (2) | US11052350B2 (fr) |
EP (1) | EP3528932B1 (fr) |
JP (1) | JP7232179B2 (fr) |
CN (1) | CN109890485B (fr) |
DE (1) | DE102016012722A1 (fr) |
WO (1) | WO2018077781A1 (fr) |
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DE102016012722A1 (de) | 2016-10-24 | 2018-04-26 | Fresenius Medical Care Deutschland Gmbh | Verfahren zur Bestimmung einer Permeationseigenschaft von Hohlfasermembranen |
DE102016012730A1 (de) * | 2016-10-24 | 2018-04-26 | Fresenius Medical Care Deutschland Gmbh | Verfahren zur Bestimmung einer Permeationseigenschaft von Hohlfasermembranen |
KR102342446B1 (ko) * | 2018-10-18 | 2021-12-22 | 주식회사 엘지화학 | 분리막 엘리먼트의 결함 검출 방법 및 분리막 엘리먼트 결함 검출 장치 |
CN110639367B (zh) * | 2019-10-25 | 2023-10-13 | 华南理工大学 | 一种非接触式中空纤维膜渗透量的测量方法和装置 |
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CN109890485A (zh) | 2019-06-14 |
DE102016012722A1 (de) | 2018-04-26 |
US20210316252A1 (en) | 2021-10-14 |
US11541355B2 (en) | 2023-01-03 |
JP2019532807A (ja) | 2019-11-14 |
US11052350B2 (en) | 2021-07-06 |
EP3528932A1 (fr) | 2019-08-28 |
CN109890485B (zh) | 2021-12-21 |
EP3528932B1 (fr) | 2023-11-29 |
JP7232179B2 (ja) | 2023-03-02 |
US20190240625A1 (en) | 2019-08-08 |
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